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1H-Indene, 2,3-dihydro-1,1,3,3,5-pentamethyl- → HCID 18177854, 화합물

HRID 394920
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인쇄 미리보기

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HRID 394920 반응식
[CH3:1][C:2]1([CH3:14])[C:10]2[C:5](=[CH:6][C:7]([CH3:11])=[CH:8][CH:9]=2)[C:4]([CH3:13])([CH3:12])[CH2:3]1.[Br:15]N1C(=O)CCC1=O>C(Cl)(Cl)(Cl)Cl.N(C(C)(C)C#N)=NC(C)(C)C#N>[Br:15][CH2:11][C:7]1[CH:6]=[C:5]2[C:10](=[CH:9][CH:8]=1)[C:2]([CH3:14])([CH3:1])[CH2:3][C:4]2([CH3:13])[CH3:12]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 664691H-Indene, 2,3-dihydro-1,1,3,3,5-pentamethyl-HCID 67184N-bromobutanimide

생성물 1

HCID 18177854HCID 18177854, 화합물수율 97.3%

시약·촉매·용매 2

HCID 6547Azobisisobutyronitrile촉매HCID 5943Carbon Tetrachloride용매

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온도
0 °C

실험 절차

10.0 g of 1,1,3,3,5-pentamethylindane were dissolved in 125 ml of carbontetrachloride and were added to the resulting solution, 9.92 g of N-bromosuccinimide and 35 mg of 2,2′-azobisisobutyronitrile (AIBN). The reaction mixture was heated to reflux for 5 hours. The reaction was cooled to 0° C. and the succinimide was filtered off. The resulting solution was concentrated in vacuo and the residue (14.7 g) was further dissolved in 150 ml of hexane. The precipitate was again removed by filtration and the solution was concentrated in vacuo, giving 13.8 g of 5-bromomethyl-1,1,3,3-tetramethylindane as a yellow oil.

후처리

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 5 hours
  3. filtrationthe succinimide was filtered off
  4. concentrationThe resulting solution was concentrated in vacuo
  5. dissolutionthe residue (14.7 g) was further dissolved in 150 ml of hexane
  6. customThe precipitate was again removed by filtration
  7. concentrationthe solution was concentrated in vacuo

출처 및 근거

ORD 기록
ord-067ca15bb01347518ae9026f4b27f31b
출처 데이터셋
uspto-grants-2003_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06603012B2

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